PROCESS FOR PREPARING BIODIESEL (METHYL ESTER)
20240026238 ยท 2024-01-25
Inventors
Cpc classification
C10L2200/0476
CHEMISTRY; METALLURGY
C10L2200/029
CHEMISTRY; METALLURGY
C10L2290/547
CHEMISTRY; METALLURGY
International classification
Abstract
The present invention discloses a method for preparing biodiesel (Methyl Ester) from any kind of oil, vegetable or non-vegetable oil or used cooking oil. Further, it relates to a method for preparing biodiesel (Methyl Ester) with 100% purity which can be directly used as a fuel in cars, trucks, buses industrial and domestic purpose without any need to blend with any petroleum diesel. The present invention also discloses the biodiesel having improved cold flow properties, flash point and 57 cetane number with reduced exhaust emission where CO.sub.2 emits approx. 2.96% v/v and CO emits approx. 0.2 ppm % v/v.
Claims
1. A process for preparing biodiesel (Methyl Ester) from vegetable or non-vegetable oil (animal oil) and/or its combination thereof, wherein the method comprising the steps of: a) discharging oil as a raw from the storage tank (1) in the reactor (3) followed by discharging the steam from the boiler (2) in the reactor (3) at the temperature of 30 to 110 degrees; b) discharging vacuum from the-pump (4) to receiver tank (5) and then through condenser (6) to the reactor (3), at the pressure in the range of 150 to 750 mg/kg for about 0 to 3 Hours; wherein the moisture contents (MC) is obtained less than 0.01 to 0.05%, after processing, steering in the reactor (3) at the rpm of 60 to 75 followed by circulation of oil Through Pump about 0-2.5 hours followed by cooling from the cooling tower (7) in the reactor to reduce the temperature from about 110 to about 70 Degrees; c) conducting-transesterification step in three phases: Phase 1: (i) discharging 10-16 wt. % methanol of total weight of oil in the reactor (3) fromthe underground storage tank (8)to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9); (ii) adding 0.7-1.5% Potassium Hydroxide Pellets (Koh) or 1-4% Sodium Methoxide (CH3NaO) in the chemical receiver tank (9) and dissolving it completely in chemical receiver tank (9), followed by circulating it for about 0-60 minutes, and then discharging to the reactor (3); wherein phase 1 Continues the process for about 0-4 hours and maintained the temp. at 80 to 70 degrees centigrade; (iii) settling the mixture of reactor (3) for 0-60 minutes, prior to separating glycerin, wherein glycerin is separated via gravity, so as to obtain a biodiesel (methyl ester) approximately with 70% of purity; Phase II: (i) discharging 3-6 wt. % of methanol of total weight of oil from the underground storage tank (8) to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9); (ii) adding 0.1-0.5% Potassium Hydroxide Pellets (Koh) or 0.1-1% Sodium Methoxide (CH3NaO) in the chemical receiver tank (9) and dissolving it completely in chemical receiver tank (9), followed by circulating it for about 0-60 minutes, and then discharging to the reactor (3); where the processed oil of phase I is present; wherein phase 1 Continues the process for about 0-4 hours and maintained the temp. at 80 to 70 degree centigrade; (iii) settling the mixture of reactor (3) for 0-60 minutes, prior to separating glycerin, wherein glycerin is separated via gravity; (iv) adding 0.1-0.8% Food Grade Phosphoric Acid (concentrated 80-99%) on Total wt., where the processed oil of phase II is present in reactor (3) followed by steering and circulating it for about 0-120 minutes; (v) settling the mixture of reactor (3) for 0-60 minutes, prior to separating Soap oil, wherein so as to obtain a biodiesel (methyl ester) approximately with 100% of purity with no residue of glycerin and soap; Phase III: (i) adding light liquid paraffin (LLP) in the range of 1-25 wt. % of total weight of biodiesel (methyl ester) of phase II, from the receiver tank (11) to the chemical receiver tank (12) and then to the reactor (10); (ii) adding TBHQ (TERT BUTYL HYDROQUINONE) in the range of 0.1% to 0.5% of total weight of biodiesel (methyl ester) of phase II, to the reactor (10), where the processed oil of phase III (i) is present followed by steering in the reactor (10) at the rpm of 60 to 70 and circulating for about 0-120 minutes, wherein the phase III (i & ii) Continues the process for about 0-2 hours while maintaining the Temp. at 70 to about 65 Degrees; (iii) shifting the biodiesel (methyl ester) of phase II from reactor (3) to reactor (10); where the processed oil of phase III (I & ii) is present followed by steering in the reactor (10) at the rpm of 60 to 70 and circulating for about 0-120 minutes; (iii) draining the biodiesel (Methyl Ester) from reactor (10) to leaf filter, wherein filter mesh is 1-3 microns, followed by discharging the filtered biodiesel B100 into storage tank (13) with 100% purity.
2. The process as claimed in claim 1, wherein the vegetable oil is selected from the group comprising Soya oil, Palm oil, Palm Stearin, Used Cooking Oil, Jatropha oil, Tallow and Sunflower oil etc.
3. The process as claimed in claim 1, wherein the weight ratio of methanol to the oil in the phase I is used approximately in the range of 1:0.10-1:0.16.
4. The process as claimed in claim 1, wherein the weight ratio of methanol to the oil in the phase II is used in the range of 1:0.03-1:0.06.
5. The process as claimed in claim 1, wherein the weight ratio of Potassium Hydroxide to the oil in the phase I is used approximately in the range of 1:0.007-1:0.015.
6. The process as claimed in claim 1, wherein the weight ratio of Sodium Methoxide to the oil in the phase I is used approximately in the range of 1:0.01-1:0.04.
7. The process as claimed in claim 1, wherein weight ratio of Potassium Hydroxide to the oil in the phase II is in the range of 1:0.001-1:0.005.
8. The process as claimed in claim 1, wherein the weight ratio of Sodium Methoxide to the oil in the phase II is used in the range of 1:0.001-1:0.01.
9. The process as claimed in claim 1, the weight ratio of Light Liquid paraffin oil to the biodiesel (methyl ester) of phase III is used in the range of 1:0.01-1:0.25.
10. The process as claimed in claim 1, wherein the weight ratio of TERT BUTYL HYDROQUINONE to the biodiesel (methyl ester) of phase III is used in the range of 1:0.001-1:0.005.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0048] Embodiments of the present invention will hereinafter be described in conjunction with the following drawings, wherein:
[0049]
[0050] The above summary, as well as the following detailed description of certain embodiments of the present invention, will be better understood when read in conjunction with the appended drawings. For the purpose of illustrating the invention, certain embodiments are shown in the drawings. It should be understood, however, that the present invention is not limited to the arrangements and instrumentality shown in the attached drawings.
DETAILED DESCRIPTION OF THE INVENTION
[0051] Accordingly, the present invention provides a method for preparing biodiesel (Methyl Ester) from vegetable or non-vegetable oil and/or its combination thereof, wherein the said method comprising the steps of: [0052] a) discharging oil as a raw from the storage tank (1) in the reactor (3) followed by discharging the steam from the boiler (2) in the reactor (3) at the temperature of 30 to 110 Degrees; [0053] b) discharging vacuum from the-pump (4) to receiver tank (5) and then through condenser (6) to the reactor (3), at the pressure in the range of 150 to 750 mg/kg for about 0 to 3 Hours; [0054] Wherein the moisture contents (MC) is obtained less than 0.01 to 0.05%, after processing, steering in the reactor (3) at the rpm of 60 to 75 followed by circulation of oil Through Pump about 0-2.5 hours followed by cooling from the cooling tower (7) in the reactor to reduce the temperature from about 110 to about 70 Degrees; [0055] C) conducting-transesterification step in three phases:
Phase 1:
[0056] (i) discharging 10-16 wt. % methanol of total weight of oil in the reactor (3) fromthe underground storage tank (8)to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9); [0057] (ii) adding 0.7-1.5% Potassium Hydroxide Pellets (Koh) or 1-4% Sodium Methoxide (CH3NaO) in the chemical receiver tank (9) and dissolving it completely in chemical receiver tank (9), followed by circulating it for about 0-60 minutes, and then discharging to the reactor (3); wherein phase 1 Continues the process for about 0-4 hours and maintained the temp. at 80 to 70 degree centigrade; [0058] (iii) settling the mixture of reactor (3) for 0-60 minutes, prior to separating glycerin, wherein glycerin is separated via gravity, so as to obtain a biodiesel (methyl ester) approximately with 70% of purity;
Phase II:
[0059] (i) discharging 3-6 wt. % of methanol of total weight of oil from the underground storage tank (8) to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9); [0060] (ii) adding 0.1-0.5% Potassium Hydroxide Pellets (Koh) or 0.1-1% Sodium Methoxide (CH3NaO) in the chemical receiver tank (9) and dissolving it completely in chemical receiver tank (9), followed by circulating it for about 0-60 minutes, and then discharging to the reactor (3); where the processed oil of phase I is present; wherein phase 1 Continues the process for about 0-4 hours and maintained the temp. at 80 to 70 degree centigrade; [0061] (iii) settling the mixture of reactor (3) for 0-60 minutes, prior to separating glycerin, wherein glycerin is separated via gravity; [0062] (iv) adding 0.1-0.8% Food Grade Phosphoric Acid (concentrated 80-99%) on Total wt., where the processed oil of phase II is present in reactor (3) followed by steering and circulating it for about 0-120 minutes; [0063] (v) settling the mixture of reactor (3) for 0-60 minutes, prior to separating Soap oil, wherein so as to obtain a biodiesel (methyl ester) approximately with 100% of purity with no residue of glycerin and soap.
Phase III:
[0064] (i) adding light liquid paraffin (LLP) in the range of 1-25 wt. % of total weight of biodiesel (methyl ester) of phase II, from the receiver tank (11) to the chemical receiver tank (12) and then to the reactor (10); [0065] (ii) adding TBHQ (TERT BUTYL HYDROQUINONE) in the range of 0.1% to 0.5% of total weight of biodiesel (methyl ester) of phase II, to the reactor (10), where the processed oil of phase III (i) is present followed by steering in the reactor (10) at the rpm of 60 to 70 and circulating for about 0-120 minutes, wherein the phase III (i & ii) Continues the process for about 0-2 hours while maintaining the Temp. at 70 to about 65 Degrees; [0066] (iii) shifting the biodiesel (methyl ester) of phase II from reactor (3) to reactor (10); where the processed oil of phase III (I & ii) is present followed by steering in the reactor (10) at the rpm of 60 to 70 and circulating for about 0-120 minutes. [0067] (iv) draining the biodiesel (Methyl Ester) from reactor (10) to leaf filter, wherein filter mesh is 1-3 microns, followed by discharging the filtered biodiesel B100 into storage tank (13) with 100% purity.
[0068] In an embodiment of the present invention, the vegetable oil is selected from the group comprising Soya oil, Palm oil, Palm Stearin, Used Cooking Oil, Jatropha oil, Tallow and Sunflower oil etc.
[0069] In another embodiment of the present invention, the weight ratio of methanol to the oil in the phase I is approximately 1:0.10-1:0.16.
[0070] In yet another embodiment of the present invention, the weight ratio of methanol to the oil in the phase II is in the range of 1:0.03-1:0.06.
[0071] In still another embodiment of the present invention, the weight ratio of Potassium Hydroxide to the oil in the phase I is approximately 1:0.007-1:0.015.
[0072] In still another embodiment of the present invention, the weight ratio of Sodium Methoxide to the oil in the phase I is approximately 1:0.01-1:0.04.
[0073] In still another embodiment of the present invention, the weight ratio of Potassium Hydroxide to the oil in the phase II is in the range of 1:0.001-1:0.005.
[0074] In still another embodiment of the present invention, the weight ratio of Sodium Methoxide to the oil in the phase II is in the range of 1:0.001-1:0.01.
[0075] In still another embodiment of the present invention, the weight ratio of Light Liquid paraffin oil to the biodiesel (methyl ester) of phase III is in the range of 1:0.01-1:0.25.
[0076] In still another embodiment of the present invention, the weight ratio of TERT BUTYL HYDROQUINONE to the biodiesel (methyl ester) of phase III is in the range of 1:0.001-1:0.005.
[0077] The ensuing description provides the methods and product only, and is not intended to limit the scope, applicability, or configuration of the claims. Rather, the ensuing description will provide those skilled in the art with an enabling description for implementing the embodiments. It is being understood that various changes may be made in the process in terms of conditions towards temperature, pressure etc. without departing from the scope of the appended claims.
[0078] The following examples are given by way of illustration of the present invention and should not be construed to limit the scope of present invention.
Example1
[0079] Phase I, II & III experiments are performed in the following manners. [0080] A. discharging used cooking oil at room temperature as a raw from the storage tank (1) in the reactor (3); Discharge the steam from the boiler (2) in the reactor (3) at the temperature up 15 to 150 Degrees. [0081] B. vacuum discharge from the-pump (4) to receiver tank (5), from receiver tank (5) Through condenser (6) to the reactor (3), Vacuum at the pressure in the range of up to 750 mg/kg up to 4 Hours. [0082] C. Wherein the moisture contents (MC) is obtained less than 0.01%, after processing, steering in the reactor (3) at the rpm up to 75 followed by circulation of oil through pump up to 2.5 hours followed by cooling from the cooling tower (7) in the reactor to reduce the temperature from 150 to 100 Degrees. [0083] D. conducting-transesterification step in three phases:
Phase 1:
[0084] 1. adischarging 18 wt. % methanol of total weight of oil in the reactor (3) fromthe underground storage tank (8)to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9). [0085] 2. Adding 2.5 wt. % Potassium Hydroxide Pellets (Koh) in the chemical receiver tank (9) And completely dissolve in chemical receiver tank (9), followed by circulation, Duration for 60 minutes, then dischargeto the reactor (3). Phase 1 Continued the process for 4 hours and maintained Temp. at 150 degrees. [0086] SettlingShut down the power and settling up to 60 minutes, Prior to separating glycerin, separating glycerin via gravity, so as to obtain a biodiesel (methyl ester) approximately with 70% of purity;
Phase II:
[0087] 1. discharging 6 wt. % methanol of total weight of oil in the reactor (3) from the underground storage tank (8) to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9). [0088] 2. Adding 1.5% Potassium Hydroxide Pellets (Koh) in the chemical receiver tank (9) And completely dissolve in chemical receiver tank (9), followed by circulation, Duration about up to 60 minutes, then discharge to the reactor (3) where the processed oil of phase I is present; [0089] Phase II Continued the process up to 3 hours and maintained Temp. at 150 degrees. [0090] SettlingShut down the power and settling for 60 minutes, prior to separating glycerin, separating glycerin via gravity, After Glycerin Separated, [0091] Adding (Food Grade Phosphoric Acid concentrated 80-99%), 0.03% on Total wt., where the processed oil of phase II is present in reactor (3); steering and circulation for 120 minutes. After completing of 120 minutes. [0092] settlingShut down the power and settling for 60 minutes, prior to separating Soap Oil. so as to obtain a biodiesel (methyl ester and glycerin and soap being separated out;
Phase III:
[0093] AAdding light liquid paraffin 5 wt. % of total weight of biodiesel (methyl ester) of phase II, from the receiver tank (11) to the chemical receiver tank (12) and then to the reactor (10). [0094] BAdding TBHQ (TERT BUTYL HYDROQUINONE) 0.02% of total weight of biodiesel (methyl ester) of phase II, to the reactor (10), where the processed oil of phase III (A) is present, steering in the reactor (10) at the rpm of 70 followed by circulation of 120 minutes. [0095] Phase III (A&B) Continued the process for 2 hours and maintained Temp. at 100 Degrees. After complete the process A&B shifting the biodiesel (methyl ester) of phase II from reactor (3) to reactor (10); where the processed oil of phase III (A&B) is present, steering in the reactor (10) at the rpm of 70 followed by circulation of 120 minutes. [0096] Process is completed.
[0097] Conclusion: We could not obtain biodiesel with 100% purity
Example2
[0098] Phase I, II & III experiments are performed in the following manners. [0099] A. Heating Palm stearin at the temperature of 90 deg, to form a liquid. [0100] B. discharging oil as a raw from the storage tank (1) in the reactor (3); Discharge the steam from the boiler (2) in the reactor (3) at the temperature of 130 Degrees. [0101] C. vacuum discharge from the-pump (4) to receiver tank (5), from receiver tank (5) Through condenser (6) to the reactor (3), vacuum at the pressure of 750 mg/kg for 4 Hours. [0102] D. Wherein the moisture contents (MC) is obtained less than 0.05%, after processing, steering in the reactor (3) at the rpm of 75 followed by circulation of oil through Pump for 2.5 hours followed by cooling from the cooling tower (7) in the reactor to reduce the temperature from 130 to 90 Degrees. [0103] E. conducting-transesterification step in three phases:
Phase 1:
[0104] 1. adischarging 17 wt % methanol of total weight of oil in the reactor (3) fromthe underground storage tank (8)to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9). [0105] 2. Adding 4% Sodium Methoxide (CH3NaO), in the chemical receiver tank (9) and completely dissolve in chemical receiver tank (9), followed by circulation, Duration for 60 minutes, then dischargeto the reactor (3). Phase 1 Continued the process for 4 hours and maintained Temp. at 130 [0106] 3. [0107] SettlingShut down the power and settling for 60 minutes, Prior to separating glycerin, separating glycerin via gravity, so as to obtain a biodiesel (methyl ester) approximately with 70% of purity;
Phase II:
[0108] adischarging 5 wt. % methanol of total weight of oil in the reactor (3) from the underground storage tank (8) to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9). [0109] Adding 2% Sodium Methoxide (CH3NaO) in the chemical receiver tank (9) And completely dissolve in chemical receiver tank (9), followed by circulation, Duration for 60 minutes, then discharge to the reactor (3) where the processed oil of phase I is present; [0110] Phase II Continued the process for a hours and maintained Temp. at 130 degree. [0111] SettlingShut down the power and settling for 60 minutes, prior to separating glycerin, separating glycerin via gravity, After Glycerin Separated, [0112] Adding (Food Grade Phosphoric Acid concentrated 80-99%), 0.4% on total wt., where the processed oil of phase II is present in reactor (3); steering and circulation 120 minutes. After completing of 120 minutes. [0113] settlingShut down the power and settling 60 minutes, prior to separating Soap Oil. so as to obtain a biodiesel (methyl ester) and glycerin and soap being separated out;
Phase III:
[0114] AAdding light liquid paraffin 10 wt. % of total weight of biodiesel (methyl ester) of phase II, from the receiver tank (11) to the chemical receiver tank (12) and then to the reactor (10). [0115] BAdding TBHQ (TERT BUTYL HYDROQUINONE) 0.1% of total weight of biodiesel (methyl ester) of phase II, to the reactor (10), where the processed oil of phase III (A) is present, steering in the reactor (10) at the rpm of 70 followed by circulation for 120 minutes. [0116] Phase III (A&B) Continued the process for 2 hours and maintained Temp. at 90 Degrees. After complete the process A&B shifting the biodiesel (methyl ester) of phase II from reactor (3) to reactor (10); where the processed oil of phase III (A&B) is present, steering in the reactor (10) at the rpm of 70 followed by circulation for 120 minutes. [0117] Process is completed.
[0118] Conclusion: Result is failed, we could not obtain biodiesel with 100% purity
Example3
[0119] Phase I, II & III experiments are performed in the following manners. [0120] A. Heating Tallow oil (animal oil) at the temperature of 90 deg, to form a liquid. [0121] B. discharging oil as a raw from the storage tank (1) in the reactor (3); Discharge the steam from the boiler (2) in the reactor (3) at the temperature of 120 Degrees. [0122] C. vacuum discharge from the-pump (4) to receiver tank (5), from receiver tank (5) Through condenser (6) to the reactor (3), Vacuum at the pressure at 750 mg/kg for 4 Hours. [0123] D. Wherein the moisture contents (MC) is obtained less than 0.05%, after processing, steering in the reactor (3) at the rpm 75 followed by circulation of oil through Pump for 2.5 hours followed by cooling from the cooling tower (7) in the reactor to reduce the temperature from 120 to 90 Degrees. [0124] E. conducting-transesterification step in three phases:
Phase 1:
[0125] 1. discharging 16th % methanol of total weight of oil in the reactor (3) fromthe underground storage tank (8) to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9). [0126] 2. Adding 1.5% Potassium Hydroxide Pellets (Kohin the chemical receiver tank (9) And completely dissolve in chemical receiver tank (9), followed by circulation, Duration for 60 minutes, then dischargeto the reactor (3). Phase 1 Continued the process for 4 hours and maintained Temp. at 120 degree. [0127] SettlingShut down the power and settling for 60 minutes, Prior to separating glycerin, separating glycerin via gravity, so as to obtain a biodiesel (methyl ester) approximately with 70% of purity;
Phase II:
[0128] 1. discharging 4 wt. % methanol of total weight of oil in the reactor (3) from the underground storage tank (8) to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9). [0129] 2. Add 1% Potassium Hydroxide Pellets (Koh) in the chemical receiver tank (9) And completely dissolve in chemical receiver tank (9), followed by circulation, Duration for 60 minutes, then discharge to the reactor (3) where the processed oil of phase I is present; [0130] Phase II Continued the process for 3 hours and maintained Temp. at 120 degree. [0131] SettlingShut down the power and settling for 60 minutes, prior to separating glycerin, separating glycerin via gravity, After Glycerin Separated, [0132] Adding (Food Grade Phosphoric Acid concentrated 80-99%) 0.8% on total wt., where the processed oil of phase II is present in reactor (3); steering and circulation for 120 minutes. After completing of 120 minutes. [0133] settlingShut down the power and settling for 60 minutes, prior to separating Soap Oil. so as to obtain a biodiesel (methyl ester) and glycerin and soap being separated out;
Phase III:
[0134] AAdding light liquid paraffin of 15 wt. % of total weight of biodiesel (methyl ester) of phase II, from the receiver tank (11) to the chemical receiver tank (12) and then to the reactor (10). [0135] BAdding TBHQ (TERT BUTYL HYDROQUINONE 0.035% of total weight of biodiesel (methyl ester) of phase II, to the reactor (10), where the processed oil of phase III (A) is present, steering in the reactor (10) at the rpm of 70 followed by circulation of 120 minutes. [0136] Phase III (A&B) Continued the process for 2 hours and maintained Temp. at 90 Degrees. After completing the process A&B. [0137] shifting the biodiesel (methyl ester) of phase II from reactor (3) to reactor (10); where the processed oil of phase III (A&B) is present, steering in the reactor (10) at the rpm of 70 followed by circulation of 120 minutes. [0138] Process is completed.
[0139] Conclusion: We could not obtain biodiesel with 100% purity
Example4
[0140] Phase I, II & III experiments are performed in the following manners. [0141] A. Heating Soya fatty at the temperature of 90 deg, to form a liquid. [0142] B. discharging oil as a raw from the storage tank (1) in the reactor (3); Discharge the steam from the boiler (2) in the reactor (3) at the temperature of 110 Degrees. [0143] C. vacuum discharge from the-pump (4) to receiver tank (5), from receiver tank (5) Through condenser (6) to the reactor (3), Vacuum at the pressure in the range of 750 mg/kg for 4 Hours. [0144] D. Wherein the moisture contents (MC) is obtained less than 0.05%, after processing, steering in the reactor (3) at the rpm of 75 followed by circulation of oil through pump 2.5 hours followed by cooling from the cooling tower (7) in the reactor to reduce the temperature from about 110 to about 80 Degrees. [0145] E. conducting-transesterification step in three phases:
Phase 1:
[0146] 1. discharging 15 wt. % methanol of total weight of oil in the reactor (3) fromthe underground storage tank (8)to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9). [0147] 2. Adding 2% Sodium Methoxide (CH3NaO), in the chemical receiver tank (9) And completely dissolve in chemical receiver tank (9), followed by circulation, Duration for 60 minutes, then dischargeto the reactor (3). Phase 1 Continued the process for 4 hours and maintained temp. at 110. [0148] SettlingShut down the power and settling for 60 minutes, Prior to separating glycerin, separating glycerin via gravity, so as to obtain a biodiesel (methyl ester) approximately with 70% of purity;
Phase II:
[0149] discharging 4 wt. % methanol of total weight of oil in the reactor (3) from the underground storage tank (8) to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9). [0150] Adding 1% Sodium Methoxide (CH3NaO) in the chemical receiver tank (9) And completely dissolve in chemical receiver tank (9), followed by circulation, Duration for 60 minutes, then discharge to the reactor (3) where the processed oil of phase I is present; [0151] Phase II Continued the process for 3 hours and maintained Temp. at 110 to 80 degree. [0152] SettlingShut down the power and settling for 60 minutes, prior to separating glycerin, separating glycerin via gravity, after glycerin Separated, [0153] Adding (Food Grade Phosphoric Acid concentrated 80-99%) 0.5% on total wt., where the processed oil of phase II is present in reactor (3); steering and circulation for 120 minutes. After completing of 120 minutes. [0154] settlingShut down the power and settling for 60 minutes, prior to separating Soap Oil. so as to obtain a biodiesel (methyl ester) and glycerin and soap being separated out;
Phase III:
[0155] AAdding light liquid paraffin in the range of 20 wt. % of total weight of biodiesel (methyl ester) of phase II, from the receiver tank (11) to the chemical receiver tank (12) and then to the reactor (10). [0156] BAdding TBHQ (TERT BUTYL HYDROQUINONE) of 0.045% of total weight of biodiesel (methyl ester) of phase II, to the reactor (10), where the processed oil of phase III (A) is present, steering in the reactor (10) at the rpm of 70 followed by circulation of 120 minutes. [0157] Phase III (A&B) continued the process for 2 hours and maintained Temp. at 110 Degrees. After completing the process, A&B. [0158] shifting the biodiesel (methyl ester) of phase II from reactor (3) to reactor (10); where the processed oil of phase III (A&B) is present, steering in the reactor (10) at the rpm of 70 followed by circulation of 120 minutes. [0159] Process is completed.
[0160] Conclusion: We obtained 100% pure biodiesel with the improved cold flow properties, however the emission control of CO2 and CO was not so good.
Example5
[0161] Phase I, II & III experiments are performed in the following manners. [0162] a) discharging sunflower fatty oil as a raw from the storage tank (1) in the reactor (3) followed by discharging the steam from the boiler (2) in the reactor (3) at the temperature of 110 Degrees; [0163] b) discharging vacuum from the-pump (4) to receiver tank (5) and then through condenser (6) to the reactor (3), at the pressure in the range of 750 mg/kg for about 2 Hours; [0164] wherein the moisture contents (MC) is obtained 0.04%, after processing, steering in the reactor (3) at the rpm of 75 followed by circulation of oil through Pump for 2 hours followed by cooling from the cooling tower (7) in the reactor to reduce the temperature from 110 to 70 Degrees; [0165] C) conducting-transesterification step in three phases:
Phase 1:
[0166] (i) discharging 15 wt. % methanol of total weight of oil in the reactor (3) fromthe underground storage tank (8)to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9); [0167] (ii) adding 1% Potassium Hydroxide Pellets (Koh) in the chemical receiver tank (9) and dissolving it completely in chemical receiver tank (9), followed by circulating it for about 45 minutes, and then discharging to the reactor (3); wherein phase 1 Continues the process for about 3.5 hours and maintained the temp. at 80 degree centigrade; [0168] (iii) settling the mixture of reactor (3) for 45 minutes, prior to separating glycerin, wherein glycerin is separated via gravity, so as to obtain a biodiesel (methyl ester) approximately with 70% of purity;
Phase II:
[0169] (i) discharging 5 wt. % of methanol of total weight of oil from the underground storage tank (8) to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9); [0170] (ii) adding 0.3% Potassium Hydroxide Pellets (Koh) in the chemical receiver tank (9) and dissolving it completely in chemical receiver tank (9), followed by circulating it for about 45 minutes, and then discharging to the reactor (3); where the processed oil of phase I is present; wherein phase 1 Continues the process for about 2.5 hours and maintained the temp. at 80 degree centigrade; [0171] (iii) settling the mixture of reactor (3) for 45 minutes, prior to separating glycerin, wherein glycerin is separated via gravity; [0172] (iv) adding 0.4% Food Grade Phosphoric Acid (concentrated 80-99%) on Total wt., where the processed oil of phase II is present in reactor (3) followed by steering and circulating it for about 90 minutes; [0173] (v) settling the mixture of reactor (3) for 45 minutes, prior to separating Soap oil, wherein so as to obtain a biodiesel (methyl ester)
Phase III:
[0174] (i) adding light liquid paraffin (LLP) in the range of 25 wt. % of total weight of biodiesel (methyl ester) of phase II, from the receiver tank (11) to the chemical receiver tank (12) and then to the reactor (10); [0175] (ii) adding TBHQ (TERT BUTYL HYDROQUINONE) in the range of 0.35% of total weight of biodiesel (methyl ester) of phase II, to the reactor (10), where the processed oil of phase III (i) is present followed by steering in the reactor (10) at the rpm of 70 and circulating for about 90 minutes, wherein the phase III (i & ii) Continues the process for about 2 hours while maintaining the Temp. at 70 degrees; [0176] (iii) shifting the biodiesel (methyl ester) of phase II from reactor (3) to reactor (10); where the processed oil of phase III (I & ii) is present followed by steering in the reactor (10) at the rpm of 60 and circulating for 120 minutes.
[0177] Conclusion: We obtained biodiesel approximately with 100% of purity with no residue of glycerin and soap. Also, cold flow properties and control of Emission achieved.
[0178] The below test report is shown the conclusion:
TABLE-US-00002 CUSTOMER DETAILS Customer Name & Address: Mr. MOHAMMED IDRIS AHMED, 6-54/15. Bank Colony Pothireddypally, Sangareddy - 502295. Customer Reference: Test Requested Form dated on 27 Jun. 2022 Test Report No: TR2206131-01 Date: 08 Jul. 2022 Page 1 of 2 SAMPLE DETAILS Sampled by: CaRE Laboratory Sampled on: 28 Jun. 2022 Sample Code: 2206131-01 Sampling Procedure: CaRE/QA/SOP/005 Sample Name: BIODIESEL (B100) Sample Received on: 28 Jun. 2022 Sample Description: Stack Emission Sample Completed on: 8 Jul. 2022 Identification by Customer DG Set 500 Location CaRE Laboratory, Kelambakkam, Chennai Identification MULTI FEED STOCK Test Results SI. No. Test Parameter Unit Test Method Results EXHAUST EMISSION PARAMETERS 1 Nitrogen as N2 %/v/v IS 5182 (Part 6): 68 2006 (Reaff: 2017) 2 Oxygen as O2 %/v/v IS 13270: 1992 11 (Reaff: 2019) 3 Carbon di-Oxide %/v/v IS 132700: 1992 2.96 as CO2 (Reaff 2019) 4 Water Vapour as %/v/v IS 5182 (Part 6): 3.0 H20 2006 (Reaff: 2017) REGULATED HARMFUL EMISSION PARAMETERS 5 Carbon %/v/v IS 13270: 1992 BDL(DL:02) monoxide as CO (Reaff: 2019) 6 Hydro carbon as PPM CPCB 56 HC Guidelines Volume-1 7 Nitrogen di- PPM IS 11255 (Part 7): 30 oxide as NOx 1985 (Reaff: 2017) 8 Sulphur di-oxide PPM IS 11255 (Part 2): 30 as SOx 1985 (Reaff: 2019) 9 Particulate PPM IS 11255 (Part 7): 40 Matter - PM 1985 (Reaff: 2019) Note: BDLBelow Detection Limit; DLDetection Limit; Test Report No: TR2206131-01 Date: 8 Jul. 2022 Page 2 of 2 SAMPLE DETAILS Sample Code: 2206131-01 Sampled on: -- Sample Name: FUEL Sampled by: Customer Sample Description: BIODIESEL Sampling Procedure: -- Identification by Customer: B100 MULTI Sample Received on: 27 Jun. 2022 FEED STOCK Test Started on: 28 Jun. 2022 Sample Completed on: 8 Jul.2022 TEST RESULTS Permissible Test Limits as SI. NO. Parameter Test Method Results Unit perASTM6751 1 Viscosity ASTMD445 4.4 Cst 3.5-5.0 @40 2 Density @ 15 ASTMD1298 0.873 Kg/m2 0.860-0.900 3 Flash point ASTMD93 149 C. >100 4 Calorific Inhouse 10080 KJ/kg >9500 value Method (BombCalorie) 5 Cetane ASTMD613 57 >51 number 6 Acid value ASTMD664 0.35 mgKOH/g >0.8 7 Cloud point ASTMD2500 3 C. 8 Pour Point ASTMD97 2 C. 9 Water content ASTMD2709 0.5 Mg/kg <500 10 Sulphur ASTMD5453 1.1 Mg/kg Max. 10 11 Total EN12662 14 Mg/kg <20 contamination 12 Copper strip ASTMD130 No. 1 Rating Class 1 corrosion, 3 hr at 50 C. 13 Methanol EN14110 0.01 % by mass <0.02 content 14 Oxidation EN14112 6.4 hr >5 Stabilityat 110 C. 15 Iodine Value ASTMD2274 44.3 g/100 g <120 16 Phosphorous ASTMD4951 0.6 Mg/kg <10 Content 17 Ester content EN14103 98.7 % by mass >96.5 18 Alkaline EN14109 3.0 Mg/kg <5 matter (NaK) 19 Alkaline EN14538 3.0 Mg/kg <5 matter (CaMg) 20 Cold Filter EN116 5 0 Plugging Point (CFPP) *** End of Test Report ***
[0179] The above test was also compared with the biodiesel obtained from the Applicant's own Patent Application No. 201641014608 and found that the present biodiesel obtained from the disclosed process is much capable in reducing exhaust emission in vehicle. A test report for biodiesel of the Patent Application No. 201641014608 on exhaust emission is given below:
TABLE-US-00003 TEST REPORT Customer Name & Address: M/s PIK BIOFUELS PRIVATE LIMITED, PLOT.NO.39, NEAR ROCK W001., MANDAL KOHIR, MEDAK DISTRICT-502321, TELANGANA, INDIA. Test Report: TR16030391B-01 Date: 12 Apr. 2016 Page 1 of 2 Customer Reference: Mail Confirmation on 9 Apr. 2016 SAMPLE DETAILS Sampled by: Client Sampled on: 11 Apr. 2016 (14:05 Hrs to 15:05 Hrs) Sample Code: 16030391B-01 Sampling Procedure: IS 5182 Part V & XIV Sample Name: Exhaust Emission Sample Received on: 11 Apr. 2016 Sample Description: Biodiesel-Animal Sample Completed on: 12 Apr. 2016 Tallow Temperature: 35.1 C. Relative Humidity: 55% Method of S.No Description Reference Units Results Exhaust Emission Components 1. Nitrogen as N2 IS 5182 (Part- % v/v 71 6)2006(R 2012) 2. Oxygen as O2 IS 13270: 1992 % v/v 11.2 (Reaff. 2009) 3. Carbon di IS 13270: 1992 % v/V 4.8 Oxide as Co2 (Reaff. 2009) 4. H20 IS 5182 (Part- % v/v 3.5 6)2006(R 2012) Regulated Harmful Components 5. Carbon IS 13270: 1992 % v/v BDL (DL:02) monoxide as (Reaff. 2009) CO 6. Hydro carbons CPCB ppm 58 as HC Guidelines Volume-1 7. Nitrogen di- IS 11255 (Part- ppm 36 oxide as NOx 7)2005(Reaff. 2012) 8. Sulphur di- IS 11255 (Part- ppm 32 oxide as SOx 2) 1985 (Reaff. 2009) 9. Particulate IS 11255 (Part- ppm 45 Matter - PM 1): 1985 (Reaff. 2009) *** Contd *** Test Report: TR16030391B-01 Date: 12 Apr. 2016 Page 2 of 2 Unregulated Harmful Components 10. Ammonia CPCB Mg/km 1.17 Guidelines Volume-1 11. Cyanides CPCB Mg/km 0.620 Guidelines Volume-1 12. Benzene as IS 5182 (Part Mg/km 3.70 C6H6 11) 2006 (R 2012) 13. Toluene IS 5182 (Part Mg/km 1.20 11) 2006 (R 2012) 14. Aldehydes CPCB Mg/km 0.0 Guidelines Volume-1 Note: BDLBelow Detection Limit; DLDetection Limit *** End of Test Report ***
Example6
[0180] Phase I, II & III experiments are performed in the following manners. [0181] d) discharging palm fatty oil as a raw from the storage tank (1) in the reactor (3) followed by discharging the steam from the boiler (2) in the reactor (3) at the temperature of 110 Degrees; [0182] e) discharging vacuum from the-pump (4) to receiver tank (5) and then through condenser (6) to the reactor (3), at the pressure in the range of 750 mg/kg for about 2 Hours; [0183] wherein the moisture contents (MC) is obtained 0.04%, after processing, steering in the reactor (3) at the rpm of 75 followed by circulation of oil through Pump for 2 hours followed by cooling from the cooling tower (7) in the reactor to reduce the temperature from 110 to 70 Degrees; [0184] f) conducting-transesterification step in three phases:
Phase 1:
[0185] (i) discharging 15 wt. % methanol of total weight of oil in the reactor (3) fromthe underground storage tank (8)to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9); [0186] (ii) adding 1.5% Sodium Methoxide (CH3NaO) in the chemical receiver tank (9) and dissolving it completely in chemical receiver tank (9), followed by circulating it for about 45 minutes, and then discharging to the reactor (3); wherein phase 1 Continues the process for about 3.5 hours and maintained the temp. at 70 degree centigrade; [0187] (iii) settling the mixture of reactor (3) for 45 minutes, prior to separating glycerin, wherein glycerin is separated via gravity, so as to obtain a biodiesel (methyl ester) approximately with 70% of purity;
Phase II:
[0188] (iv) discharging 5 wt. % of methanol of total weight of oil from the underground storage tank (8) to the chemical receiver tank (9) wherein the exact quantity and accuracy of methanol is maintained by the Level Indicator in chemical receiver tank (9); [0189] (v) adding 0.35% Sodium Methoxide (CH3NaO) in the chemical receiver tank (9) and dissolving it completely in chemical receiver tank (9), followed by circulating it for about 45 minutes, and then discharging to the reactor (3); where the processed oil of phase I is present; wherein phase 1 Continues the process for about 2.5 hours and maintained the temp. at 70 degree centigrade; [0190] (vi) settling the mixture of reactor (3) for 45 minutes, prior to separating glycerin, wherein glycerin is separated via gravity; [0191] (iv) adding 0.4% Food Grade Phosphoric Acid (concentrated 80-99%) on Total wt., where the processed oil of phase II is present in reactor (3) followed by steering and circulating it for 90 minutes; [0192] (v) settling the mixture of reactor (3) for 45 minutes, prior to separating Soap oil, wherein so as to obtain a biodiesel (methyl ester)
Phase III:
[0193] (iv) adding light liquid paraffin (LLP) in the range of 25 wt. % of total weight of biodiesel (methyl ester) of phase II, from the receiver tank (11) to the chemical receiver tank (12) and then to the reactor (10); [0194] (v) adding TBHQ (TERT BUTYL HYDROQUINONE) in the range of 0.35% of total weight of biodiesel (methyl ester) of phase II, to the reactor (10), where the processed oil of phase III (i) is present followed by steering in the reactor (10) at the rpm of 70 and circulating for about 90 minutes, wherein the phase III (i & ii) Continues the process for 2 hours while maintaining the Temp. at 65 degrees; [0195] (vi) shifting the biodiesel (methyl ester) of phase II from reactor (3) to reactor (10); where the processed oil of phase III (I & ii) is present followed by steering in the reactor (10) at the rpm of and circulating for 120 minutes.
[0196] Conclusion: We obtained biodiesel approximately with 100% of purity with no residue of glycerin and soap. Also, cold flow properties and control of Emission is achieved with almost same result as above.
[0197] The same experiments of Examples 5 and 6 were performed with other fatty oils such as jatropa oil, soyabean oil, tallow oil, used cooking oil and its combination, however we achieved almost same result as concluded in Example 5.
Advantages of the Present Invention
[0198] The main advantages of the present invention are: [0199] 1) Present invention provides with cost effective biodiesel (methyl ester) prepared from the any of the vegetable or animal oil, even the used cooking oil which is easily available. [0200] 2) Present invention provides with high quality biodiesel (methyl ester) which can directly be used as a fuel without blended with any other petroleum diesel. [0201] 3) Present invention provides biodiesel (methyl ester) with reduced exhaust emission in vehicle and improved cold flow properties. [0202] 4) Present invention provides biodiesel (methyl ester) with reduced exhaust emission components and increase the level of oxygen in environment. [0203] 5) Present invention provides biodiesel (methyl ester) with reduced harmful components.